Phosphorus oxide (P4O10) → HCID 21051547, Verbindung

HRID 2213557Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2213557
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[CH2:15]([O:17][C:18]([C:20]1[C:21]([CH2:26][CH2:27][C:28]([OH:30])=O)=[CH:22][NH:23][C:24]=1[CH3:25])=[O:19])[CH3:16]>>[CH2:15]([O:17][C:18]([C:20]1[C:21]2[CH2:26][CH2:27][C:28](=[O:30])[C:22]=2[NH:23][C:24]=1[CH3:25])=[O:19])[CH3:16]

Komponenten

3

Edukt 2

HCID 14812Phosphorus oxide (P4O10)HCID 217287442-Methyl-3-carbethoxy-4-(3-propionic acid)pyrrole

Produkt 1

HCID 21051547HCID 21051547, VerbindungAusbeute 85 %

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Polyphosphoric acid (20 g) and P2O5 (1.0 g) were mixed together and heated at 70° C. for 20 min. To the mixture was added 3-(4-ethoxycarbonyl-5-methyl-3-pyrrolyl)propanoic acid (1.0 g, 4.44 mmol) and heating was continued for 20 hours. The reaction was poured into ice-water, extracted with EtOAc. The organic layer was washed with brine and sat. NaHCO3, and dried (MgSO4). After removal of the solvent, the crude product was recrystallized from CH2CI2-hexane to give (0.78 g, 85%) of 2-methyl-6-oxo-1,4,5,6-tetrahydro-cyclopenta[b]pyrrole-3-carboxylic acid ethyl ester as a white solid.

Aufarbeitung

  1. temperatureheating
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine and sat. NaHCO3
  4. dry with materialdried (MgSO4)
  5. customAfter removal of the solvent
  6. customthe crude product was recrystallized from CH2CI2-hexane

Quellen und Nachweise

ORD-Eintrag
ord-d14de4fd13ce47d0a1166ac42444dd83
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07105562B2

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